CN101708402B - Multiphase nitride combined silicon carbide ceramic foam filter and preparation method thereof - Google Patents
Multiphase nitride combined silicon carbide ceramic foam filter and preparation method thereof Download PDFInfo
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- CN101708402B CN101708402B CN2009102276265A CN200910227626A CN101708402B CN 101708402 B CN101708402 B CN 101708402B CN 2009102276265 A CN2009102276265 A CN 2009102276265A CN 200910227626 A CN200910227626 A CN 200910227626A CN 101708402 B CN101708402 B CN 101708402B
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Abstract
The invention relates to a multiphase nitride combined silicon carbide ceramic foam filter and a preparation method thereof, and belongs to the technical field of refractory materials. The preparation method is realized in a way as follows: preparing slurry from silicon, silicon carbide, silicon dioxide, ball clay, admixtures and water; soaking the slurry by using soft polyurethane foam as the carrier to prepare a blank; and drying, and sintering at 1400-1500 DEG C in the nitrogen atmosphere to obtain the multiphase nitride combined silicon carbide ceramic foam filter. The ceramic foam filterof the invention has favorable high temperature stability in ferric and copper solutions, does not pollute alloys, has the open-cell rate of 80-90%, has favorable filtration and adsorption capacitieson oxide inclusions and flux inclusions, and has the advantages of high filter capacity, favorable filtration and purifying effect, small hot melt and high thermal shock stability; the compression strength at normal temperature is not lower than 2.3 MPa; the ceramic foam filter can be cooled by water at 1100-20 DEG C for more than 23 times, and does not need preheating in use; and the highest service temperature is 1550 DEG C.
Description
Technical field
The present invention relates to the purification of motlten metal, be specifically related to the foam ceramic filter technology, the present invention relates to a kind of cast iron, cast copper multiphase nitride combined silicon carbide ceramic foam filter in particular.
Background technology
The pore that produces in slag inclusion in the metal melting process and the casting cycle occupies larger specific gravity in casting defect.In Foundry Production, the casting wasted product rate that is caused by non-metallic inclusion is generally up to 50%～60% of waste product sum, adopt ceramic foam filter filtering metal liquid then can reduce the waste product that 60%～80% slag and impurity are brought into, simultaneously, improve significantly through the foundry goods mechanical performance and the cutting ability of filtering.
At present, abroad, there has been the company of some developed countries to be engaged in the production of casting with the ceramic foam filter of silicon carbide material, developed the ceramic foam filter Selee/Fe of the binding type silicon carbide material that is used to filter ferrous metal in 1984 as U.S. Consoldated Aluminum company, the specification of hole dimension is 15,25PPI, and thickness is 19～25mm.The U.S. has also succeeded in developing SiC-Al
2O
3Composite slug type magnesium iron filters and uses ceramic foam filter, and it consists of 50%SiC, 40%Al
2O
3, all the other are sintering aid, binding agent etc.
Day this product river white refining watt company also produces with SiC and Si
3N
4For the foamed ceramics of material is crossed device.Pottery Co., Ltd of Japan Toshiba (Toshiba) is with Si in the ceramic foam filter patent to German application in 1987
3N
4Be material, add the Al more than 1%
2O
3, SiO
2, TiO
2, MgO, ZrO and Cr
2O
3Deng as sintering aid, its sintering temperature is 1500～1800 ℃, and bulk density is 0.7g/cm
3, compressive resistance is 11MPa; When no sintering aid, compressive resistance has only 1MPa.
The famous Foseco company of Britain has just successfully developed the silicon carbide foam ceramic filter (model is Sedex) that filters most of cast iron, part high-melting-point copper alloy in the early stage eighties in 20th century.The silicon carbide foam ceramic filter that these companies produced is produced the needs except that satisfying this country, also occupies the bigger market share in China, its good product quality, but cost an arm and a leg.
Shenyang Research Institute of Foundry also develops the cast iron ceramic foam filter, and its open pore rate is 80%, and bulk density is 0.4g/cm3, and the highest cast temperature is 1400 ℃, and it crosses flow rate is 15kg/cm
2Min.
The SiC foam ceramic filter of Dong Feng Auto Corporation's exploitation, wherein (W (SiC)=45%, W (Al
2O
3)=45%), its bore dia is plurality of specifications such as 10ppi, 20ppi, thickness is 22mm, can improve the quality of spheroidal graphite cast-iron, gray iron, malleable iron foundry goods, help to slow down the turbulence level of watering molten iron in the road junction, have good thermal shock resistance and elevated temperature strength, can bear the extreme environment in the cast iron process.
Every performance indications of the silicon carbide foam ceramic filter that is used for the cast iron industry that the basic new material of Jincheng City richness limited company produces are as follows: hole density (ppi): 4-60; Through-hole rate (%): 80-90; Maximum operation (service) temperature (℃): 1500; Normal temperature bending strength (Mpa): 0.8; Normal temperature compressed intensity (Mpa): 0.8; Thermal shock resistance (inferior/1100 ℃): 6
Chinese patent 1830911A is with carborundum, aluminium oxide, clay, water, and does the adhesive preparation slip with dextrin and Ludox, prepared 1500 ℃ of maximum operation (service) temperatures, and through-hole rate is 80%～90%, and unit weight is 0.5～0.65g/cm
3, 1100 ℃～20 ℃ water-cooleds, the oxide combined silicon carbide ceramic foam filter that does not split for 20 times.
Chinese patent 101164655A is with carborundum, aluminium oxide, silica, talcum and water, and make bond with carboxymethyl cellulose, polyvinyl alcohol and Ludox and prepare slip, having prepared through-hole rate is 80%～90%, the aperture is the oxide combined silicon carbide ceramic foam filter of 10PPI, this filter has good high-temperature stability in iron, copper solution, do not pollute alloy, oxide inclusion in the metallic solution and flux are mingled with good filtration and adsorption capacity.
Chinese patent 1700948A has prepared the oxide combined silicon carbide ceramic foam filter with the ceramic mud of the fumed silica of carborundum, cataloid bond and at least 10%.
Be used for high temperature resistant silicon carbide foam ceramic filters such as cast iron and continuous casting, also do not form production scale at present, what have is in the development phase, the import in a large number of required product.According to customs statistics, only the siliceous filter of the carbonization of calendar year 2001 PORT OF TIANJIN import just reaches 2,000 ten thousand.
Summary of the invention
It is good to the purpose of this invention is to provide a kind of elevated temperature strength, can bear big flow molten hot metal and wash away and anxious thermal shock, and the multiphase nitride combined silicon carbide ceramic foam filter that thermo-chemical stability is good is to be suitable for the filtration, purification of iron and ferrous alloy; A kind of preparation method of above-mentioned multiphase nitride combined silicon carbide ceramic foam filter is provided, makes the filter that makes have good sintering and comprehensive physical property, and have good thermal shock resistance.
The multiphase nitride combined silicon carbide ceramic foam filter that the present invention proposes is as raw material with silicon, carborundum, silica and ball clay and additive; Wherein the mass content of silicon is 19～45%, and the mass content of carborundum is 39～65%, and the mass content of silica is 5～11%, and the mass content of ball clay is 3～5%; The mass content of additive is 0.5%～1.3%; Described additive comprises carboxymethyl cellulose, sodium humate and water reducer F10; The thing phase composition of described ceramic foam filter comprises silicon nitride, silicon oxynitride and carborundum; Wherein the total amount of silicon nitride and silicon oxynitride is 38%～70%, and the content of silicon oxynitride is 3～10%.
The preparation method of described multiphase nitride combined silicon carbide ceramic foam filter, with carborundum is principal crystalline phase, adopts the silicon nitride that reaction in-situ generates under nitrogen atmosphere to make multiphase nitride combined silicon carbide ceramic foam filter with silicon oxynitride mutually for combination; Specific embodiment is: with silicon, carborundum, silica and ball clay and additive and water prepare slurry, with the flexible polyurethane foams is carrier, flood above-mentioned slurry, extruding, and compressed air blown is removed surperficial plug-hole, make base substrate, base substrate is packed in the sintering furnace, under nitrogen atmosphere, programming rate with 60 ℃/h rises to 600 ℃ by room temperature, and is incubated 1～2h under this temperature, treat foamed plastics burning volatilization after, programming rate with 300 ℃/h rises to 1200 ℃ again, and under this temperature, be incubated 2h～5h, rise to 1300 ℃ with the programming rate of 50 ℃/h, and under this temperature, be incubated 2h～4h, programming rate with 50 ℃/h rises to 1400～1500 ℃, and is incubated 2h～4h under this temperature; Obtain multiphase nitride combined silicon carbide ceramic foam filter.
In sum, the existing silicon carbide foam ceramic filter material oxide combined silicon carbide that all is sintering in oxidizing atmosphere.Silicon carbide foam ceramic filter material of the present invention is complex phase silicon nitride and the silicon oxynitride based on silicon carbide that reaction in-situ generates, by introducing silica flour in slip, sintering preparation under high pure nitrogen atmosphere.Because nitride has better mechanics, thermal property, has given better mechanical property of material and thermal shock resistance.
The multiphase nitride combined silicon carbide ceramic foam filter of the present invention's preparation is the space network structure, wherein hole interconnects, through-hole rate can reach 80～90%, the convection cell resistance is little, in iron, copper solution, has good high-temperature stability, do not pollute alloy, oxide inclusion in the metallic solution and flux are mingled with good filtration and adsorption capacity, cold crushing strength is not less than 2.3MPa, filtration yield is big, and filtration, purification is effective, and hot melt is little, thermal shock resistance is very high, and 1100 ℃～20 ℃ water-cooleds are greater than 23 times; Can preheating during use; Maximum operation (service) temperature is 1550 ℃.
Following table has been listed the performance of domestic and imported foam silicon carbide ceramics filter, and and the performance of the multiphase nitride combined silicon carbide ceramic foam filter of the present invention's development compares, as can be seen, the ceramic foam filter of the present invention's development has higher compression strength and better thermal shock resistance, and serviceability temperature is higher 50 ℃ than existing ceramic filter.
| Performance | Homemade ceramic filter | The import ceramic filter | The invention ceramic filter |
| Maximum operation (service) temperature | 1500℃ | 1500℃ | 1550℃ |
| Porosity | 80％～85％ | 80％～90％ | 85％～90％ |
| Unit weight | 0.5～0.65 | 0.45～0.65 | 0.4～0.6 |
| Compression strength | 0.8MPa | 1.6MPa | 2.3MPa |
| Thermal shock resistance | 1100 ℃～20 ℃ water-cooleds are not split for 6 times | 1100 ℃～20 ℃ water-cooleds are not split for 20 times | 1100 ℃～20 ℃ water-cooleds are not split for 23 times |
The specific embodiment
Embodiment 1
According to 19: 65: 11: 5 weight ratio fully was mixed and made into ceramic powders with silicon, carborundum, silica, ball clay.
With ceramic powders, carboxymethyl cellulose, sodium humate, F10 and water according to 100: 0.5: 0.2: 0.3: 60 weight ratio is mixed, and adding with the aluminium oxide is ball milling 3～5h in the polyurethane ball grinder of abrasive media, makes ceramic size.
Select the flexible polyurethane foams of 10PPI for use, be processed into 60mm * 60mm * 20mm size, as the carrier of ceramic slurry.
Carrier is immersed in the ceramic size prepare in advance, treat that carrier is filled slip after, extrude unnecessary slip, compressed then air blown is removed surperficial plug-hole, makes the ceramic foam filter base substrate.
The ceramic foam filter base substrate is put into drying box, earlier at 60 ℃ of insulation 4～6h, again 100～120 ℃ of dry sclerosis of insulation 20～24h.
Dried base substrate is packed in the sintering furnace, under nitrogen atmosphere, programming rate with 60 ℃/h rises to 600 ℃ by room temperature, and under this temperature, be incubated 2h, after treating foamed plastics burning volatilization, programming rate with 300 ℃/h rises to 1200 ℃ again, and under this temperature, be incubated 1h, programming rate with 50 ℃/h rises to 1300 ℃, and under this temperature, be incubated 2h, rise to 1400 ℃ with the programming rate of 50 ℃/h, and under this temperature, be incubated 4h, naturally cool to room temperature and come out of the stove, can obtain multiphase nitride combined silicon carbide ceramic foam filter.Use XRD analysis, obtain the thing phase composition and be: wherein the total amount of silicon nitride and silicon oxynitride is 38%, and wherein the content of silicon nitride is 35%, and the content of silicon oxynitride is 3%.
Embodiment 2
According to 29: 56: 11: 4 weight ratio fully was mixed and made into ceramic powders with silicon, carborundum, silica, ball clay.
With ceramic powders, carboxymethyl cellulose, sodium humate, F10 and water according to 100: 0.3: 0.15: 0.4: 55 weight ratio is mixed, and adding with the aluminium oxide is ball milling 3～5h in the polyurethane ball grinder of abrasive media, makes ceramic size.
Select the flexible polyurethane foams of 10PPI for use, be processed into 60mm * 60mm * 20mm size, as the carrier of ceramic slurry.
Carrier is immersed in the ceramic size prepare in advance, treat that carrier is filled slip after, extrude unnecessary slip, compressed then air blown is removed surperficial plug-hole, makes the ceramic foam filter base substrate.
The ceramic foam filter base substrate is put into drying box, earlier at 60 ℃ of insulation 4～6h, again 100～120 ℃ of dry sclerosis of insulation 20～24h.
Dried base substrate is packed in the sintering furnace, under nitrogen atmosphere, programming rate with 60 ℃/h rises to 600 ℃ by room temperature, and under this temperature, be incubated 2h, after treating foamed plastics burning volatilization, programming rate with 300 ℃/h rises to 1200 ℃ again, and under this temperature, be incubated 4h, programming rate with 50 ℃/h rises to 1300 ℃, and under this temperature, be incubated 3h, rise to 1450 ℃ with the programming rate of 50 ℃/h, and under this temperature, be incubated 3h, naturally cool to room temperature and come out of the stove, can obtain multiphase nitride combined silicon carbide ceramic foam filter.Wherein the total amount of silicon nitride and silicon oxynitride is 50～55%, and wherein the content of silicon nitride is 40～45%, and the content of silicon oxynitride is 10%.
Embodiment 3
According to 36: 56: 5: 3 weight ratio fully was mixed and made into ceramic powders with silicon, carborundum, silica, ball clay.
With ceramic powders, carboxymethyl cellulose, sodium humate, F10 and water according to 100: 0.2: 0.15: 0.3: 50 weight ratio is mixed, and adding with the aluminium oxide is ball milling 3～5h in the polyurethane ball grinder of abrasive media, makes ceramic size.
Select the flexible polyurethane foams of 10PPI for use, be processed into 60mm * 60mm * 20mm size, as the carrier of ceramic slurry.
Carrier is immersed in the ceramic size prepare in advance, treat that carrier is filled slip after, extrude unnecessary slip, compressed then air blown is removed surperficial plug-hole, makes the ceramic foam filter base substrate.
The ceramic foam filter base substrate is put into drying box, earlier at 60 ℃ of insulation 4～6h, again 100～120 ℃ of dry sclerosis of insulation 20～24h.
Dried base substrate is packed in the sintering furnace, under nitrogen atmosphere, programming rate with 60 ℃/h rises to 600 ℃ by room temperature, and under this temperature, be incubated 2h, after treating foamed plastics burning volatilization, programming rate with 300 ℃/h rises to 1200 ℃ again, and under this temperature, be incubated 5h, programming rate with 50 ℃/h rises to 1300 ℃, and under this temperature, be incubated 2h, rise to 1500 ℃ with the programming rate of 50 ℃/h, and under this temperature, be incubated 2h, naturally cool to room temperature and come out of the stove, can obtain multiphase nitride combined silicon carbide ceramic foam filter.Wherein the total amount of silicon nitride and silicon oxynitride is 55～65%, and wherein the content of silicon nitride is 50%～55%, and the content of silicon oxynitride is 5～10%.
Embodiment 4
According to 45: 39: 11: 5 weight ratio fully was mixed and made into ceramic powders with silicon, carborundum, silica, ball clay.
With ceramic powders, carboxymethyl cellulose, sodium humate, F10 and water according to 100: 0.4: 0.15: 0.5: 50 weight ratio is mixed, and adding with the aluminium oxide is ball milling 3～5h in the polyurethane ball grinder of abrasive media, makes ceramic size.
Select the flexible polyurethane foams of 10PPI for use, be processed into 60mm * 60mm * 20mm size, as the carrier of ceramic slurry.
Carrier is immersed in the ceramic size prepare in advance, treat that carrier is filled slip after, extrude unnecessary slip, compressed then air blown is removed surperficial plug-hole, makes the ceramic foam filter base substrate.
The ceramic foam filter base substrate is put into drying box, earlier at 60 ℃ of insulation 4～6h, again 100～120 ℃ of dry sclerosis of insulation 20～24h.
Dried base substrate is packed in the sintering furnace, under nitrogen atmosphere, programming rate with 60 ℃/h rises to 600 ℃ by room temperature, and under this temperature, be incubated 2h, after treating foamed plastics burning volatilization, programming rate with 300 ℃/h rises to 1200 ℃ again, and under this temperature, be incubated 2h, programming rate with 50 ℃/h rises to 1300 ℃, and under this temperature, be incubated 2h, rise to 1500 ℃ with the programming rate of 50 ℃/h, and under this temperature, be incubated 2h, naturally cool to room temperature and come out of the stove, can obtain multiphase nitride combined silicon carbide ceramic foam filter.Wherein the total amount of silicon nitride and silicon oxynitride is 65～70%, and wherein the content of silicon nitride is 60～65%, and the content of silicon oxynitride is 5%.
Claims (3)
1. multiphase nitride combined silicon carbide ceramic foam filter is characterized in that: described ceramic filter is as raw material with silicon, carborundum, silica and ball clay and additive; Wherein the mass content of silicon is 19～45%, and the mass content of carborundum is 39～65%, and the mass content of silica is 5～11%, and the mass content of ball clay is 3～5%; The mass content of additive is 0.5%～1.3%; Described additive comprises carboxymethyl cellulose, sodium humate and water reducer F10; The thing phase composition of described ceramic foam filter comprises silicon nitride, silicon oxynitride and carborundum; Wherein the total amount of silicon nitride and silicon oxynitride is 38%～70%, and the content of silicon oxynitride is 3～10%.
2. multiphase nitride combined silicon carbide ceramic foam filter according to claim 1, it is characterized in that: the addition of described carboxymethyl cellulose is not more than 0.3%, the addition of sodium humate is not more than 0.5%, and the addition of water reducer F10 is not more than 0.5%.
3. the method for preparing the described multiphase nitride combined silicon carbide ceramic foam filter of claim 1, it is characterized in that: be principal crystalline phase with carborundum, adopt the silicon nitride that reaction in-situ generates under nitrogen atmosphere to make multiphase nitride combined silicon carbide ceramic foam filter mutually for combination with silicon oxynitride; Specific embodiment is: with silicon, carborundum, silica and ball clay are formed ceramic powders, add the additive carboxymethyl cellulose again, sodium humate, water reducer F10 and water prepare slurry, with the flexible polyurethane foams is carrier, flood above-mentioned slurry, unnecessary slurry is got rid of in extruding earlier, and thereby compressed air is blown away surperficial plug-hole and is made base substrate, base substrate is packed in the sintering furnace, under nitrogen atmosphere, programming rate with 60 ℃/h rises to 600 ℃ by room temperature, and is incubated 1～2h under this temperature, treat foamed plastics burning volatilization after, programming rate with 300 ℃/h rises to 1200 ℃ again, and under this temperature, be incubated 2h～5h, rise to 1300 ℃ with the programming rate of 50 ℃/h, and under this temperature, be incubated 2h～4h, programming rate with 50 ℃/h rises to 1400～1500 ℃, and is incubated 2h～4h under this temperature; Obtain multiphase nitride combined silicon carbide ceramic foam filter.
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| CN101708402B true CN101708402B (en) | 2011-05-25 |
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